WO2010038281A1 - Zeolite separation membrane, process for producing the same, and binder - Google Patents
Zeolite separation membrane, process for producing the same, and binder Download PDFInfo
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- WO2010038281A1 WO2010038281A1 PCT/JP2008/067797 JP2008067797W WO2010038281A1 WO 2010038281 A1 WO2010038281 A1 WO 2010038281A1 JP 2008067797 W JP2008067797 W JP 2008067797W WO 2010038281 A1 WO2010038281 A1 WO 2010038281A1
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- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/003—Membrane bonding or sealing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
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- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
- B01D71/0281—Zeolites
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
- C04B37/005—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of glass or ceramic material
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/04—Specific sealing means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/04—Specific sealing means
- B01D2313/041—Gaskets or O-rings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D2313/042—Adhesives or glues
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/04—Ceramic interlayers
- C04B2237/06—Oxidic interlayers
- C04B2237/062—Oxidic interlayers based on silica or silicates
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/10—Glass interlayers, e.g. frit or flux
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
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- C04B2237/343—Alumina or aluminates
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/76—Forming laminates or joined articles comprising at least one member in the form other than a sheet or disc, e.g. two tubes or a tube and a sheet or disc
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/88—Joining of two substrates, where a substantial part of the joining material is present outside of the joint, leading to an outside joining of the joint
Abstract
Description
によって形成することが好ましい。 In the method for producing a zeolite separation membrane according to the present invention, it is preferable to form a zeolite layer on the surface of the ceramic porous tube by hydrothermal synthesis.
1)セラミック多孔質管と接合部材の固着
(a)図3において、セラミック多孔質管(1)(アルミナ99%、外径16mmφ、内径12mmφ)を封止するために、同管(1)の一端部と封止栓(3)(緻密質アルミナ)との間に、ガラス粉末を圧縮成型したガラスリング(2)を介在させた(図3a参照)。ここで使用したガラス粉末の組成は、表2中のBに示すものである。次いで、これを900℃で1時間焼成することにより、管(1)の一端部を封止した構造を得た。 Example 1
1) Adhesion of ceramic porous tube and joining member
(a) In FIG. 3, in order to seal the ceramic porous tube (1) (alumina 99%,
図4において、上記のように一端部に封止栓をガラスにて固着させたセラミック多孔質管を、A型ゼオライト結晶粒子(東ソー社製ゼオラム)の懸濁液(0.10wt%)に浸漬した。ゼオライト結晶粒子を担持したセラミック多孔質管端部を2時間室温で放置した後、37℃で1晩乾燥した。次に、これらのゼオライト担持端部を反応ゲル液(組成Na2O:SiO2:Al2O3:H2O = 88:100:4:3960)に浸漬した状態で、100℃で4時間水熱合成を行った。この水熱合成によりセラミック多孔質管の外表面にゼオライト膜が形成された。 2) Synthesis of Zeolite Separation Membrane In FIG. 4, a ceramic porous tube having a sealing stopper fixed to one end with glass as described above is used as a suspension of A-type zeolite crystal particles (Zeolam manufactured by Tosoh Corporation) (0.10 wt%). The end of the ceramic porous tube carrying the zeolite crystal particles was left at room temperature for 2 hours and then dried at 37 ° C. overnight. Next, these zeolite-supported ends were immersed in a reaction gel solution (composition Na 2 O: SiO 2 : Al 2 O 3 : H 2 O = 88: 100: 4: 3960) at 100 ° C. for 4 hours. Hydrothermal synthesis was performed. By this hydrothermal synthesis, a zeolite membrane was formed on the outer surface of the ceramic porous tube.
エタノール/水 = 90wt% / 10wt%
反応温度 = 75℃
下記の式に従って分離係数を求めた。 PV test conditions: Effective membrane area 10.1cm 2
Ethanol / water = 90wt% / 10wt%
Reaction temperature = 75 ℃
The separation factor was determined according to the following formula.
CWater : 水の濃度
CEtOH : エタノール濃度
得られた試験結果は下記の通りである。 Separation factor = (C Water / C EtOH ) permeation side / (C Water / C EtOH ) supply side
C Water : Water concentration C EtOH : Ethanol concentration
The test results obtained are as follows.
図4(b)のゼオライト分離膜:分離係数1381
この結果から、図4(a)のゼオライト分離膜および図4(b)のゼオライト分離膜はいずれも、接合部のシールが極めて高い気密性を有するとともに、同シールはゼオライト分離膜に対して影響をほとんど及ぼさないことがわかる。 Fig. 4 (a) Zeolite separation membrane: Separation factor 9986
Fig. 4 (b) zeolite separation membrane: separation factor 1381
From this result, both the zeolite separation membrane of FIG. 4 (a) and the zeolite separation membrane of FIG. 4 (b) have a very high airtightness at the joint, and the seal has an influence on the zeolite separation membrane. It can be seen that it hardly affects.
下記の方法でガラス粉末への安定化ジルコニア添加の効果を調べた。 Example 2
The effect of adding stabilized zirconia to glass powder was investigated by the following method.
下記の方法でガラス粉末組成が膜性能へ及ぼす影響を調べた。 Example 3
The effect of glass powder composition on film performance was investigated by the following method.
下記の方法で接合部材の組成及び熱膨張係数がコーテイング状況(密着性・気密性)に及ぼす影響を調べた。 Example 4
The effects of the composition and thermal expansion coefficient of the joining member on the coating situation (adhesion and airtightness) were investigated by the following methods.
セラミック多孔質管の端部構造と接合部材の端部構造の変形例を図7(a)(b)(c)(d)に示す。図中、(1)はセラミック多孔質管、(2)は接合剤、(3)は封止栓、(4)はガラスコーティング、(18)は封止キャップ、(21)は接合部材である。 Example 5
7 (a) (b) (c) (d) show modified examples of the end structure of the ceramic porous tube and the end structure of the joining member. In the figure, (1) is a ceramic porous tube, (2) is a bonding agent, (3) is a sealing plug, (4) is a glass coating, (18) is a sealing cap, and (21) is a bonding member. .
(2) ガラスリング
(3) 封止栓
(4) ガラスコーティング
(5) 溶融ガラス層
(6) ゼオライト層
(18) 封止キャップ
(21) 接合部材 (1) Ceramic porous tube (2) Glass ring (3) Seal plug (4) Glass coating (5) Molten glass layer (6) Zeolite layer (18) Sealing cap (21) Joining member
Claims (11)
- 主成分としてアルミナで構成される多孔質管と、同管との接合位置に配された接合部材とが、必須成分としてSiO2:17~48wt%、Al2O3:2~8wt%、BaO:24~60wt%、ZnO:0.5~5wt%を含み、かつLa2O3、CaOおよびSrOのうち少なくとも1つを含むセラミックの酸化物からなる接合剤によって固着され、多孔質管の表面にゼオライト薄層が形成されてなることを特徴とする分離膜。 A porous tube composed of alumina as a main component and a joining member arranged at the joining position with the tube are, as essential components, SiO 2 : 17 to 48 wt%, Al 2 O 3 : 2 to 8 wt%, BaO : 24 to 60 wt%, ZnO: 0.5 to 5 wt%, and fixed on the surface of the porous tube by a bonding agent made of a ceramic oxide containing at least one of La 2 O 3 , CaO and SrO. A separation membrane comprising a thin layer.
- 接合部材が、セラミック多孔質管の少なくとも一端を封止する封止栓であるか、または、セラミック多孔質管の少なくとも一端に接合される管であることを特徴とする請求項1記載の分離膜。 The separation membrane according to claim 1, wherein the joining member is a sealing plug for sealing at least one end of the ceramic porous tube, or a tube joined to at least one end of the ceramic porous tube. .
- 接合部材の端部とセラミック多孔質管の端部が嵌合されていることを特徴とする請求項1記載の分離膜。 2. The separation membrane according to claim 1, wherein an end of the joining member and an end of the ceramic porous tube are fitted.
- 接合部材の熱膨張係数が4~9 x 10-6 (/K)であることを特徴とする請求項1記載の分離膜。 2. The separation membrane according to claim 1, wherein the joining member has a thermal expansion coefficient of 4 to 9 × 10 −6 (/ K).
- 接合部材が、主成分としてアルミナ50wt%以上を含有し、セラミックの酸化物の割合が0.1~40wt%であり、結晶粒径が1μm以上であることを請求項1記載の分離膜。 2. The separation membrane according to claim 1, wherein the joining member contains 50 wt% or more of alumina as a main component, the ratio of ceramic oxide is 0.1 to 40 wt%, and the crystal grain size is 1 μm or more.
- 主成分としてアルミナで構成される多孔質管と、同管に接合すべき接合部材とを接合位置に配し、必須成分としてSiO2:17~48wt%、Al2O3:2~8wt%、BaO:24~60wt%、ZnO:0.5~5wt%を含み、かつLa2O3、CaOおよびSrOのうち少なくとも1つを含むセラミックの酸化物からなる接合剤を多孔質管と接合部材の間に介在させ、接合剤を焼成することによって多孔質管と接合部材を固着し、その後多孔質管の表面にゼオライト層を形成することを特徴とする分離膜の製造方法。 A porous tube composed of alumina as a main component and a bonding member to be bonded to the tube are arranged at the bonding position. As essential components, SiO 2 : 17 to 48 wt%, Al 2 O 3 : 2 to 8 wt%, BaO: 24 to 60 wt%, ZnO: 0.5 to 5 wt%, and a bonding agent comprising a ceramic oxide containing at least one of La 2 O 3 , CaO and SrO is interposed between the porous tube and the bonding member A method for producing a separation membrane, comprising interposing and bonding a porous tube and a bonding member by firing a bonding agent, and then forming a zeolite layer on the surface of the porous tube.
- 接合剤を、セラミックの酸化物粉末の成型品の形態でまたは同酸化物粉末を含むスラリーの形態で、多孔質管と接合部材の間に介在させ、接合剤を焼成することによって多孔質管と接合部材を固着することを特徴とする請求項6記載の分離膜の製造方法。 The bonding agent is interposed between the porous tube and the bonding member in the form of a ceramic oxide powder molded product or in the form of a slurry containing the oxide powder, and the bonding agent is fired to form the porous tube. The method for producing a separation membrane according to claim 6, wherein the joining member is fixed.
- セラミックの酸化物粉末の成型品がバインダを含むか、または成型品がバインダを含み成型後に焼成によってバインダを除去したものであることを特徴とする請求項7記載の分離膜の製造方法。 8. The method for producing a separation membrane according to claim 7, wherein the molded product of ceramic oxide powder contains a binder, or the molded product contains a binder and the binder is removed by firing after molding.
- セラミック多孔質管の表面にゼオライト層を水熱合成によって形成するに際して、水熱合成の前に、ゼオライト粒子を懸濁させた懸濁液にセラミック多孔質管を浸漬し乾燥させることによって、ゼオライト粒子を多孔質管の表面に付着させることを特徴とする請求項8記載の分離膜の製造方法。 When the zeolite layer is formed on the surface of the ceramic porous tube by hydrothermal synthesis, before the hydrothermal synthesis, the ceramic porous tube is dipped in a suspension in which the zeolite particles are suspended, and dried. The method for producing a separation membrane according to claim 8, wherein the is attached to the surface of the porous tube.
- 主成分としてアルミナで構成される多孔質管と接合部材とを接合させるための接合剤であって、必須成分としてSiO2:17~48wt%、Al2O3:2~8wt%、BaO:24~60wt%、ZnO:0.5~5wt%を含み、かつLa2O3、CaOおよびSrOのうち少なくとも1つを含むセラミックの酸化物からなることを特徴とする接合剤。 It is a bonding agent for bonding a porous tube composed of alumina as a main component and a bonding member. As essential components, SiO 2 : 17 to 48 wt%, Al 2 O 3 : 2 to 8 wt%, BaO: 24 A bonding agent comprising: 60 wt%, ZnO: 0.5 to 5 wt%, and comprising a ceramic oxide containing at least one of La 2 O 3 , CaO and SrO.
- 接合剤がさらにイットリアによって安定化させたジルコニアを0.1~20wt%含むことを特徴とする請求項10記載の接合剤。 The bonding agent according to claim 10, further comprising 0.1 to 20 wt% of zirconia stabilized by yttria.
Priority Applications (4)
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EP08877140.7A EP2343115A4 (en) | 2008-10-01 | 2008-10-01 | Zeolite separation membrane, process for producing the same, and binder |
CN200880131379.2A CN102170962B (en) | 2008-10-01 | 2008-10-01 | Zeolitic separation membrane, its manufacture method and binding agent |
PCT/JP2008/067797 WO2010038281A1 (en) | 2008-10-01 | 2008-10-01 | Zeolite separation membrane, process for producing the same, and binder |
US12/998,221 US9022226B2 (en) | 2008-10-01 | 2008-10-01 | Zeolite separation membrane, method for producing the same, and bonding agent |
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PCT/JP2008/067797 WO2010038281A1 (en) | 2008-10-01 | 2008-10-01 | Zeolite separation membrane, process for producing the same, and binder |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012008476A1 (en) * | 2010-07-14 | 2012-01-19 | 日本碍子株式会社 | Ceramic filter |
CN106116663A (en) * | 2016-07-05 | 2016-11-16 | 山东理工大学 | Filter-type activated carbon lead zinc is prepared porous and is catchmented the method for sponge brick |
CN106116664A (en) * | 2016-07-05 | 2016-11-16 | 山东理工大学 | Absorbent-type Maifanitum sand Rhizoma Zingiberis Recens soil potter's clay microballon is prepared porous and is catchmented the method for sponge brick |
CN106146014A (en) * | 2016-07-05 | 2016-11-23 | 山东理工大学 | Filter-type activated carbon Iron-ore Slag is prepared porous and is catchmented the method for sponge brick |
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AT15049U1 (en) * | 2015-12-21 | 2016-11-15 | Plansee Se | Membrane arrangement with bonding layer |
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CN106116663A (en) * | 2016-07-05 | 2016-11-16 | 山东理工大学 | Filter-type activated carbon lead zinc is prepared porous and is catchmented the method for sponge brick |
CN106116664A (en) * | 2016-07-05 | 2016-11-16 | 山东理工大学 | Absorbent-type Maifanitum sand Rhizoma Zingiberis Recens soil potter's clay microballon is prepared porous and is catchmented the method for sponge brick |
CN106146014A (en) * | 2016-07-05 | 2016-11-23 | 山东理工大学 | Filter-type activated carbon Iron-ore Slag is prepared porous and is catchmented the method for sponge brick |
Also Published As
Publication number | Publication date |
---|---|
US20110174722A1 (en) | 2011-07-21 |
CN102170962B (en) | 2016-01-06 |
US9022226B2 (en) | 2015-05-05 |
EP2343115A4 (en) | 2013-04-17 |
CN102170962A (en) | 2011-08-31 |
EP2343115A1 (en) | 2011-07-13 |
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